EP3822614B1 - Viscometer - Google Patents

Viscometer Download PDF

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Publication number
EP3822614B1
EP3822614B1 EP19834300.6A EP19834300A EP3822614B1 EP 3822614 B1 EP3822614 B1 EP 3822614B1 EP 19834300 A EP19834300 A EP 19834300A EP 3822614 B1 EP3822614 B1 EP 3822614B1
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EP
European Patent Office
Prior art keywords
measurement
sample
viscosity
stage
viscometer
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Application number
EP19834300.6A
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German (de)
English (en)
French (fr)
Other versions
EP3822614A1 (en
EP3822614A4 (en
Inventor
Hideyuki Amamiya
Yoshinori Nakashima
Keiji KAWADA
Toshio Kasai
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Atago Co Ltd
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Atago Co Ltd
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Publication date
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Publication of EP3822614A1 publication Critical patent/EP3822614A1/en
Publication of EP3822614A4 publication Critical patent/EP3822614A4/en
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N11/00—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
    • G01N11/10—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by moving a body within the material
    • G01N11/14—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by moving a body within the material by using rotary bodies, e.g. vane
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N11/00—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
    • G01N11/10—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by moving a body within the material
    • G01N11/14—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by moving a body within the material by using rotary bodies, e.g. vane
    • G01N11/142—Sample held between two members substantially perpendicular to axis of rotation, e.g. parallel plate viscometer
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B7/00—Measuring arrangements characterised by the use of electric or magnetic techniques
    • G01B7/16—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N11/00—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
    • G01N2011/0006—Calibrating, controlling or cleaning viscometers
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N11/00—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
    • G01N11/10—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by moving a body within the material
    • G01N11/14—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by moving a body within the material by using rotary bodies, e.g. vane
    • G01N11/142—Sample held between two members substantially perpendicular to axis of rotation, e.g. parallel plate viscometer
    • G01N2011/145—Sample held between two members substantially perpendicular to axis of rotation, e.g. parallel plate viscometer both members rotating
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N11/00—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
    • G01N11/10—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by moving a body within the material
    • G01N11/14—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by moving a body within the material by using rotary bodies, e.g. vane
    • G01N2011/147—Magnetic coupling

Definitions

  • the present disclosure relates to a viscometer.
  • Rotational viscometers are known that measure viscosity of a sample in a liquid state, for example, according to an equilibrium position between a reactive torque applied to a rotor rotating in the sample and a torsional reactive force of a spring with one end fixed to a rotor shaft.
  • Patent Document 1 discloses the related technique.
  • Other examples of prior art devices can be seen in JPS61132840 , US5103679 , US4622846 , JP2001272323 and CN101936868 .
  • JPS61132840 discloses a viscometer according to the preamble of claim 1.
  • Patent Document 1 Japanese Unexamined Patent Application Publication No. H09-126981
  • Conventional rotational viscometers typically need about several tens of seconds to one minute from the start of rotation of the rotor until the equilibrium position becomes stable and allows the measurement. This period of time causes an increase in temperature of the sample due to friction between the rotating rotor and the sample. The increase in temperature impedes the accurate measurement of the viscosity that greatly depends on the temperature in the conventional rotational viscometers, and should be improved so as to measure the viscosity with a higher accuracy. An improvement in accuracy of the measurement and a reduction in time for the measurement are required to improve the efficiency in sample-manufacturing facilities that need to deal with a large number of samples to measure the viscosity in a short time.
  • the present disclosure provides a viscometer capable of measuring viscosity with a high accuracy in a short time.
  • the viscometer of the invention is defined in claim 1, and its dependent claims.
  • the viscometer can measure the viscosity with a high accuracy in a short time.
  • the viscometer 51 includes a body 1 which is thin in the upper-lower direction and elongated in the front-rear direction in appearance to allow a user to hold by the hand.
  • the body 1 is provided on the front side with a stage 2 projecting upward and formed into a substantially columnar shape.
  • the measurement cap 3 is removably attached to the stage 2.
  • the attachment structure is a bayonet mount, for example.
  • the stage 2 is provided with cap engagement parts 755 to be engaged with claws (not illustrated) provided on the inner surface of the circumferential wall 32 of the measurement cap 3.
  • the measurement cap 3 is to be attached to the stage 2 such that the measurement cap 3 is pushed downward while the claws and the cap engagement parts 755 are aligned in the circumferential direction and is then rotated in the circumferential direction, as indicated by the arrow DRa in Fig. 2 .
  • the measurement cap 3 covers a measurement stage 81 in the attached state illustrated in Fig. 1 .
  • the disk-shaped measurement stage 81 is exposed when the measurement cap 3 in the measurement state is removed, as illustrated in Fig. 2 .
  • a sample mount 811 of the measurement stage 81 has a sample mount surface 811a which is horizontal in a state in which the body 1 is placed on the horizontal surface with the bottom surface in contact therewith.
  • Fig. 3 is a block diagram illustrating a functional configuration of the viscometer 51, which is also described below with reference to Fig. 3 .
  • the display 12 includes a display element 12a mounted on the board 16.
  • the display element 12a displays pieces of information such as an operating state of the viscometer 51 and a value of viscosity measured so as to allow the user to visually recognize the information.
  • the operation part 13 includes a plurality of push buttons mounted on the board 16 so that the user executes the operations of turning ON/OFF of a power supply and starting the measurement.
  • Fig. 2 illustrates a power supply button 13a and a measurement start button 13b.
  • the temperature detection part 14 includes a port 14a provided on the upper case 111, and a temperature sensor 14b mounted on the board 16 at a position corresponding to the port 14a.
  • the temperature sensor 14b measures an ambient temperature around the body 1.
  • the body 1 is provided inside with a battery housing part 15 for housing a battery BT such as a dry cell.
  • the lower case 112 is provided on the rear surface with a cap 15a openable and covering the battery housing part 15 to allow the battery BT to be replaced.
  • a controller 17 including a central processing unit (CPU) 171 and a memory 172 is mounted on the board 16.
  • CPU central processing unit
  • the measurer who uses the viscometer 51 can generally measure the viscosity of a sample through the following process.
  • the measurer first removes the measurement cap 3 and places the viscometer 51 on the horizontal surface such as a table with the bottom surface of the body 1 facing down.
  • the measurer pushes the power supply button 13a to turn on the viscometer 51.
  • the measurer puts a suitable amount of the sample on the sample mount surface 811a of the sample mount 811 of the measurement stage 81 which is exposed. The suitable amount is about 0.3 ml, for example.
  • the measurer then attaches the measurement cap 3 to the stage 2 and pushes the measurement start button 13b.
  • the pushing the measurement start button 13b causes the viscometer 51 to start the measurement.
  • the controller 17 of the viscometer 51 obtains the viscosity of the sample by a predetermined method (described below) and displays the numerical value of the viscosity obtained on the display 12.
  • the time required for the measurement from the push of the measurement start button 13b to the display of the numerical value of the viscosity is about one second.
  • Fig. 4 is a cross-sectional view taken along S4-S4 in Fig. 1 .
  • Fig. 4 is a lateral cross-sectional view of the stage 2, while illustrating a motor 71 in a side view.
  • Fig. 5 is an assembly diagram of a viscosity measurement unit 7 illustrated in Fig. 4 .
  • the configuration of the viscosity measurement unit 7 supported by the casing 11 is described in detail with reference to Fig. 4 and Fig. 5 .
  • the viscosity measurement unit 7 is also simply referred to below as a measurement unit 7.
  • the measurement unit 7 includes the motor 71, a bearing unit 72, a motor mount 73, a base 75, and a strain gauge unit 74 listed from the lower side.
  • the measurement unit 7 further includes a connection nut 76, a rotation plate 77, an O-ring 78, a waterproof plate 79, a thrust bearing 80, the measurement stage 81, and the measurement cap 3 each arranged over the base 75.
  • the motor 71 is a stepper motor, and includes a motor body 711, a shaft 713 as an output shaft, and a motor plate 712 that is a lid of the motor body 711 on the upper side.
  • the bearing unit 72 includes a sleeve 721 and a radial bearing 722.
  • the sleeve 721 has a cylindrical shape to which an inner ring (not shown) of the radial bearing 722 is fitted on the outer surface.
  • the sleeve 721 includes a male screw part 7211 provided with an external thread at the upper part.
  • the motor mount 73 includes a plate-like mount base 731, a projection 733 projecting in the middle of the mount base 731 and having a diameter tapering off with two steps, and a mount pin 732 pressure inserted in the mount base 731 to project upward.
  • the projection 733 includes a base-side projection 7331 and a tip-side projection 7332 having a smaller diameter than the base-side projection 7331.
  • the base 75 is described in detail with reference to Fig. 6 which is its perspective view.
  • the base 75 has a disk-like shape having a penetration hole 751 about an axial line CL75 extending in the upper-lower direction as a center.
  • the base 75 includes a reference surface 757, a circumferential rib 752, a recess 753, and a round groove 754.
  • the reference surface 757 is a surface as a reference of the base 75 in the direction of the axial line CL75.
  • the circumferential rib 752 projects upward along a circumferential edge of the reference surface 757.
  • the recess 753 is recessed into a circle in the middle of the reference surface 757.
  • the round groove 754 is provided on the reference surface 757.
  • the base 75 also includes the cap engagement parts 755 described above provided on the outer circumferential surface of the circumferential wall and separated from each other by 180 degrees in the circumferential direction.
  • the strain gauge unit 74 is described in detail with reference to Fig. 7 which is its perspective view. As illustrated in Fig. 7 , the strain gauge unit 74 includes a gauge part 741, a cantilever 742, and a holder 743 which are unitized.
  • the gauge part 741 is composed of a beam load cell.
  • the beam load cell used can be a commercially-available product.
  • the gauge part 741 has a substantially rectangular parallelepiped elongated in the A-B direction in Fig. 7 , and is provided with a strain gauge 741b stuck on a side surface 741a.
  • the strain gauge unit 74 outputs by the strain gauge 741b a voltage corresponding to the amount of bending deformation in the direction indicated by the arrow DRb on the B-end side opposite to the A-end side.
  • the gauge part 741 on the A-end side is fixed to the holder 743 with a screw 745.
  • the output voltage of the gauge part 741 is amplified by an amplifier 746 (refer to Fig. 2 ).
  • the voltage amplified by the amplifier 746 is monitored by the controller 17 and is stored as necessary.
  • the motor plate 712 of the motor 71 is fixed to the motor mount 73 with screws 734 and 735.
  • the shaft 713 of the motor 71 is rotatably inserted to the sleeve 721 of the bearing unit 72.
  • An outer ring (not shown) of the radial bearing 722 of the bearing unit 72 is pressure inserted and fixed to the inner surface of the tip-side projection 7332 of the projection 733 of the motor mount 73.
  • the sleeve 721 of the bearing unit 72 is inserted to the penetration hole 751 of the base 75 from the lower side with the male screw part 7211 projecting upward.
  • the connection nut 76 is fastened on the male screw part 7211 projecting upward so as to fix the bearing unit 72 to the base 75.
  • the motor 71 is thus supported, by the motor mount 73, rotatably about an axial line CL71via the radial bearing 722.
  • the shaft 713 of the motor 71 is also rotatable with respect to the motor mount 73.
  • Fig. 8 and Fig. 9 are views for explaining the arranged position of the strain gauge unit 74 with respect to the motor 71 and the like.
  • Fig. 8 is a top view illustrating an assembled state of the motor 71, the bearing unit 72, the motor mount 73, and the strain gauge unit 74.
  • the position taken along (S4)-(S4) in Fig. 8 corresponds to the cross-sectioned position shown in Fig. 4 .
  • Fig. 9 is a front view of Fig. 8 , also illustrating a part of the lower surface 756 of the base 75 in cross section to which the holder 743 of the strain gauge unit 74 is fixed.
  • the contact of the motor mount 73 rotating in the clockwise direction with the holder 743 stops the rotation of the motor 71 with substantially no deformation of the holder 743.
  • the contact of the mount pin 732 of the motor mount 73 rotating in the counterclockwise direction with the cantilever 742 further pushes the cantilever 742.
  • the gauge portion 741 is then subjected to bending deformation with the B-end side displaced in the direction indicated by the arrow DRb and the A-end side as a fixed end.
  • the gauge part 741 outputs a voltage corresponding to the amount of strain based on the deformation.
  • the measurement unit 7 thus can obtain a rotational biasing force of the motor 71 in the counterclockwise direction (indicated by the arrow DRd) in accordance with the output voltage of the strain gauge unit 74.
  • the configuration of the measurement unit 7 on the lower side of the base 75 has been described above.
  • the configuration of the measurement unit 7 on the upper side of the base 75 is described below with reference to Fig. 4 and Fig. 5 .
  • the disk-shaped rotation plate 77 is coaxially fixed to the tip of the shaft 713 projecting upward from the sleeve 721.
  • the rotation plate 77 is provided with a plurality of plate magnets 771 fitted along the circumferential edge at equal angular intervals at the same position in the radial direction with the same pole facing upward.
  • the plate magnets 771 are herein fitted in the attitude in which the N-pole faces upward.
  • the rotation plate 77 is housed in the recess 753 of the base 75 such that the upper surface 772 of the rotation plate 77 is located at a level lower than the reference surface 757 of the base 75.
  • the waterproof plate 79 is fixed to the reference surface 757 of the base 75 with screws (not shown) while pressing the O-ring 78 fitted to the round groove 754. In particular, the waterproof plate 79 pushes down the O-ring 78, which is housed in the round groove 754 while slightly projecting upward, so as to be tightly attached to the reference surface 757.
  • the inner space of the recess 753 of the base 75 keeps its watertight state against the outside due to the waterproof plate 79 tightly attached to the reference surface 757 to push down the O-ring 78 and due to the screw engagement between the sleeve 721 and the connection nut 76.
  • the measurement stage 81 is rotatably mounted on the upper surface of the waterproof plate 79 via the thrust bearing 80.
  • the measurement stage 81 has a disk-like shape to which the thrust bearing 80 is coaxially attached in the middle of the lower surface 815 of the measurement stage 81.
  • a plurality of stage magnets 814 are fitted to the lower surface 815 of the measurement stage 81 to surround the thrust bearing 80.
  • the plural stage magnets 814 are arranged such that each substantially faces one of the plate magnets 771 of the rotation plate 77 at a particular rotational position.
  • the respective stage magnets 814 are fitted to the measurement stage 81 in the attitude in which the magnetic pole on the side (the lower side) facing the plate magnets 771 is opposite to that of the plate magnets 771 so as to attract each other.
  • the stage magnets 814 are arranged in the attitude such that the magnetic pole on the lower side is the S-pole.
  • each of the stage magnets 814 is arranged to face the corresponding one of the plate magnets 771 so as to magnetically attract each other.
  • the measurement stage 81 is thus automatically aligned and positioned on the waterproof plate 79 by the magnetic attraction about the axial line CL71 serving as an axis.
  • the measurement stage 81 which is not directly connected to the rotation plate 77, is automatically coaxially positioned so as to keep the magnetic balance with the rotation plate 77 in the radial direction.
  • the measurement stage 81 is magnetically attracted to the rotation plate 77 and positioned by the thrust bearing 80 in the thrust direction.
  • a frictional resistance in the rotating direction of the measurement stage 81 is substantially negligible due to the thrust bearing 80.
  • the measurement stage 81 thus synchronously rotates substantially integrally with the rotation plate 77.
  • the upper surface of the measurement stage 81 is provided with the sample mount 811 described above having the sample mount surface 811a which is a slightly-recessed circular flat surface.
  • the sample mount 811 has a circumferential groove 813 deeply hollowed along the entire circumference on the outer side in the radial direction.
  • the part between the sample mount 811 and the circumferential groove 813 serves as a bank 812 relatively projecting upward along the entire circumference.
  • the sample mount surface 811a is opposed in parallel to a counter surface 33a of the cap stage 33 of the measurement cap 3 with a slight gap provided therebetween in the state in which the measurement cap 3 is attached to the stage 2.
  • the sample mount surface 811a and the counter surface 33a are closely opposed to each other.
  • the slight gap is set in a range of about 0.1 to 0.2 mm, for example.
  • a system including the shaft 713, the rotation plate 77, and the measurement stage 81 in the measurement unit 7 is referred to as a rotation system Ra rotating relative to the motor body 711.
  • the measurement unit 7 described in detail above is attached to the casing 11 such that the base 75 is fixed with screws (not shown) to the upper case 111 with the O-ring 114 interposed therebetween, as illustrated in Fig. 4 .
  • the casing 11 includes the upper case 111 fixed to the lower case 112 with screws (not shown) with the O-ring 113 interposed therebetween. This structure keeps the inside of the casing 11 watertight from the external space.
  • the measurement unit 7 is supported by the casing 11 such that only the base 75 is connected to the casing 11 but the other members excluding the base 75 are not in contact with the fixed member of the casing 11.
  • a sample of which the viscosity P is measured is referred to as a sample Sm.
  • the viscometer 51 with the measurement cap 3 removed is placed such that the sample mount surface 811a of the sample mount 811 horizontally faces upward.
  • the sample Sm with the amount of about 0.3 ml, for example, is put on the sample mount surface 811a, and the measurement cap 3 is attached to the base 75.
  • the controller 17 causes the display 12 to display the ambient temperature around the body 1 measured by the temperature sensor 14b.
  • the controller 17 may compensate the temperature by a known method in accordance with the measured ambient temperature so as to obtain the viscosity P.
  • Fig. 10 is an enlarged cross-sectional view of a region in a partly-omitted state including a gap between the counter surface 33a of the cap stage 33 and the sample mount surface 811a of the sample mount 811 in a state in which the sample Sm is put on the sample mount surface 811a and in which the measurement cap 3 is attached to the base 75. Attaching the measurement cap 3 keeps the sample on the sample mount surface 811a spreading in the gap in the circular part at which the sample mount surface 811a is opposed to the counter surface 33a of the cap stage 33.
  • the gap is a thin disk-shaped space having a diameter Da and a height ta.
  • the diameter Da corresponds to a diameter of the cap stage 33 which is 25 mm, for example, and the height ta corresponds to a thickness of the gap in the direction of the axial line CL71 between the counter surface 33a of the cap stage 33 and the sample mount surface 811a of the sample mount 811 which is in a range of 0.1 to 0.2 mm, for example.
  • the thin disk-shaped space in which the sample is entirely or partly filled and kept is referred to as a sample filling space Va.
  • the CPU 171 starts driving the motor 71.
  • the CPU 171 starts driving the rotation system Ra including the shaft 713 with respect to the motor body 711 under a predetermined startup condition Pt.
  • the startup condition Pt is preliminarily set such that the rotation system Ra reaches a steady-state rotation at a drive pulse speed of 5000 Hz within less than one second from the startup (for example, after about 0.8 seconds).
  • the rotating direction of the shaft 713 with respect to the motor body 711 is the clockwise direction (indicated by the arrow DRc) in the top view in Fig. 8 .
  • the startup condition Pt is preliminarily set for each type of the sample Sm, and is stored in the memory 172 while being linked with the corresponding sample Sm.
  • the startup characteristics used herein are represented by time transition of the rotation rate of the rotation system Ra.
  • the rotation system Ra does not start rotating until a torque applied thereto reaches a startup torque opposing a resistance which is caused due to a viscous stress of the sample Sm filled in the sample filling space Va.
  • the motor body 711 then rotates in the counterclockwise direction shown in Fig.
  • the rotation system Ra rotates at a steady rotation rate in the equilibrium state in which the reactive torque Tqa applied in the direction impeding the rotation is constant.
  • the shaft 713 rotates in the clockwise direction (indicated by the arrow DRc) in Fig. 8 relative to the motor body 711 due to the startup command of the CPU 171.
  • the rotation plate 77 fixed to the tip of the shaft 713, and the measurement stage 81 not connected mechanically but connected magnetically to the rotation plate 77 also rotate together.
  • the rotation system Ra is caused to start rotating after the torque in the rotating direction, which is caused by the deformation resistance of the strain gauge against the pressure of the motor body 711, reaches the startup torque which corresponds to the viscosity of the sample Sm.
  • the reactive torque Tqa in the direction impeding the rotation acts on the rotation system Ra.
  • the motor body 711 rotates in the counterclockwise direction (indicated by the arrow DRd) in Fig. 8 due to the reactive torque Tqa, and pushes the cantilever 742 backward in Fig. 8 with the force corresponding to the magnitude of the reactive torque Tqa.
  • the gauge part 741 is thus deformed backward (indicated by the arrow DRb) on the B-end side with respect to the A-end side as the fixed end and outputs the voltage corresponding to the amount of deformation.
  • Fig. 11 is a graph showing time transition characteristics VT of the output voltage V from the gauge part 741 in the startup operation of the rotation system Ra.
  • the axis of ordinates of the graph indicates the output voltage V.
  • the time transition characteristics VT show the voltage V1 in the original state in which the gauge part 741 has no strain, and show the voltage V2 during the steady-state rotation that is the equilibrium state where the strain is caused by the reactive torque Tqa applied after the startup.
  • the axis of abscissas indicates the time t.
  • the time t1 is the startup command time
  • the time t2 is the rotation start time at which the torque in the rotating direction reaches the startup torque.
  • the time t3 and the time t4 are the measurement start time and the measurement end time, respectively.
  • the CPU 171 averages the output voltages V obtained from the time t3 to the time t4, and uses the average as a reference measurement voltage V2a for obtaining the viscosity P of the sample Sm.
  • the voltage V1 is 0.610 V
  • the voltage V2 is 1.630 V.
  • the time t1 is presumed to be zero seconds
  • the time t2 is 0.824 seconds
  • the time t3 is 1.00 seconds
  • the time t4 is 1.30 seconds.
  • the memory 172 of the controller 17 is caused to link the type of the sample Sm with the corresponding startup condition Pt set for each type of the sample Sm, and stores the linked data.
  • the startup condition is set such that several viscometer-correction reference liquids having different viscosities P are used as a sample, for example, and a startup pulse speed and a drive pulse speed are determined so that the startup time (the time t2 - the time t1) of the time transition characteristics VT in Fig. 11 is less than one second for each viscosity.
  • a startup condition table TBa is then created in which the respective viscosities P, the startup conditions Pt each matched with the corresponding viscosity P, and the reference measurement voltages V2a which are obtained from the startups using the viscometer-correction reference liquids having different viscosities P as samples, are linked with each other.
  • the startup condition table TBa created is stored in the memory 172.
  • the startup condition table TBa is preferably created for each type of sample. Examples of types of samples classified include a lubricant, cooking oil, cooking source, and paint. Creating the startup condition table TBa for each type of sample and obtaining a relationship between the viscosity P and the reference measurement voltage V2a enables to estimate the viscosity P with a higher accuracy, and to choose an appropriate processing method for estimating the viscosity P depending on whether the sample is a Newtonian fluid or non-Newtonian fluid.
  • Fig. 12 illustrates an example of the startup condition table TBa.
  • the startup condition table TBa illustrated in Fig. 12 is an example of a table created such that the type of sample is a "lubricant A (Newtonian fluid)".
  • This table indicates the respective startup conditions for measuring the samples having the viscosities P1 to Pn (n is an integer of two or greater) listed in ascending order, which are matched with the corresponding startup conditions Pt1 to Ptm (m is an integer of two or greater and n or smaller).
  • the samples having the closer viscosities P can be measured under the same startup condition, such that the same startup condition Pt1 is assigned to the samples having the viscosities P1 to P3, while the startup condition Pt2 is assigned to the samples having the viscosity P4 and the followings listed below, for example, in the startup condition table TBa shown in Fig. 12 .
  • At least either the startup pulse speed or the drive pulse speed is increased for the sample having higher viscosity P, so as to adjust the startup time to less than a predetermined time (for example, less than one second).
  • the startup condition table TBa shown in Fig. 12 is set for each type of sample such that the each sample is linked with one of the reference measurement voltages V2a1 to V2an, each of which is obtained as a reference measurement voltage V2a by starting the driving the motor 71 under the startup conditions assigned to the samples having the different viscosities P1 to Pn.
  • the viscosity P and the reference measurement voltage V2a are substantially in proportional relationship.
  • the viscosity P can be estimated with a high accuracy regardless of whether the number of data measured in advance is small.
  • a relational expression Qa indicating the proportional relationship between the viscosity P and the reference measurement voltage V2a is preferably stored for each startup condition table TBa.
  • the measurer inputs the type of the sample Sm1 and the numerical value of the viscosity P4 close to the approximate estimated viscosity for the sample Sm1 via the operation unit 13 of the viscometer 51.
  • the CPU 171 refers to, among the plural startup condition tables stored in the memory 172, the startup condition table TBa (which is herein the table shown in Fig. 12 ) corresponding to the "lubricant A (Newtonian fluid), which is the type of the sample input.
  • the CPU 171 acquires the startup condition Pt2 corresponding to the viscosity P4 from the startup condition table TBa, and sets the startup condition Pt2 to be used for the subsequent measurement and stores it in the memory 172.
  • the measurer places the viscometer 51 on the horizontal surface with the bottom surface facing down.
  • the measurer then puts a predetermined amount of the sample Sm1 on the sample mount part 811, attaches the measurement cap 3 to the base 75, and pushes the measurement start button 13b.
  • the CPU 171 starts driving the rotation system Ra under the set startup condition Pt2 in response to the push of the measurement start button 13b, and stores the reference measurement voltage V2a acquired as a reference measurement voltage V2ay in the memory 172.
  • the CPU 171 compares the acquired reference measurement voltage V2ay with the reference measurement voltage V2a4 for the viscosity P4 acquired from the startup condition table TBa, substitutes the difference therebetween for the relational expression Qa to obtain the viscosity of the sample Sm1, and displays the viscosity on the display 12 while storing it in the memory 172.
  • the time from which the CPU 171 acquires the reference measurement voltage V2a1 to which the CPU 171 displays the viscosity of the sample Sm1 on the display 12 is quite short, and is about one second after the push of the measurement start button 13b.
  • the viscometer 51 also includes the strain gauge unit 74 including the cantilever 742 biased by the rotation of the motor body 711 in a first direction (indicated by the arrow DRd).
  • the viscometer 51 further includes the controller 17 including the memory 172 that stores the startup condition table TBa and the CPU 171 that controls the operation of the motor 71.
  • the controller 17 recognizes the reference measurement voltage V2a output in accordance with the amount of deformation of the strain gauge unit 74 caused by the biased cantilever 742, and refers to the startup condition table TBa to obtain the viscosity P corresponding to the reference measurement voltage V2a.
  • the controller 17 When the controller 17 starts driving the rotation system Ra including the shaft 713 and the measurement stage 81 in a second direction opposite to the first direction in the state in which the sample is filled in the sample filling space Va, the motor body 711 rotates in the first direction due to the resistance caused by the viscous stress of the sample. The motor body 711 then comes into contact with the cantilever 742 at the reactive torque Tqa corresponding to the viscous resistance, and further biases the cantilever 742 in the first direction after the rotation system Ra reaches the steady-state rotation. The controller 17 obtains the viscosity P of the sample based on the reference measurement voltage V2a immediately after the rotation system Ra reaches the steady-state rotation.
  • the viscometer 51 can measure the viscosity P in a short time.
  • the increase in temperature of the sample can be reduced to a negligible level, thus enabling to measure the viscosity P with a high accuracy.
  • the viscometer 51 which can measure the viscosity with a quite small amount of the sample, has flexibility as to the measurement location. In addition, the viscometer 51 is easy to clean after the measurement since the counter surface 33a and the sample mount surface 811a are flat and have a relatively small area. The viscometer 51 is thus easy to handle.
  • the viscometer 51 is illustrated above with a portable hand-held type including the body 1 which is holdable, the viscometer 51 may be a stationary type used such that the body 1 when measuring is placed on a table or a shelf.
  • the type of the casing 11 to which the measurement unit 7 is installed may be determined as appropriate.
  • the measurement unit 7 and the controller 17 may be separated and each provided with a communication unit to implement a system so as to communicate with each other in either a wireless or wired manner, as illustrated in Fig. 13 .
  • Fig. 13 is a diagram showing a configuration example of a viscosity measurement system 52 including a plurality of viscosity measurement units 7A1 to 7Ak arranged in the k-number lines (k is an integer of two or greater) for producing samples, and an integrated control device 17T which communicates with the respective viscosity measurement units 7A1 to 7Ak in either a wireless or wired manner.
  • the viscosity measurement units 7A1 to 7Ak each include the viscosity measurement unit 7 and a measurement-side communication unit 91.
  • the integrated control device 17T includes a control-side communication unit 92 and an integrated controller 17S.
  • the integrated controller 17S can simultaneously control the respective viscosity measurement units 7A1 to 7Ak in the same manner as the controller 17 of the viscometer 51 that controls the single viscosity measurement unit 7.
  • the integrated controller 17S displays the information of the respective viscosity measurement units 7A1 to 7Ak on an integrated display 121.
  • the respective viscosity measurement units 7A1 to 7Ak are preferably capable of automatically attaching and removing of the measurement cap 3, putting the sample on the sample mount 811, and executing the viscosity measurement including the cleaning of the measurement cap 3 and the sample mount 811 after the measurement.
  • This automatic operation can take full advantage of the functions of the viscometer 51 that can measure the viscosity with a high accuracy in a short time, so as to efficiently produce samples with high quality and less variation in viscosity.
  • the motor 71 is not limited to the stepper motor, and may be a DC motor or an AC motor instead.
  • the stepper motor has the advantage of enabling the repeated startup under the respective startup conditions Pt with a high accuracy and stability.
  • the pair of the opposed surfaces to define the sample filling space Va is not limited to the pair of the counter surface 33a and the sample mount surface 811a as described above that are the flat surfaces parallel to each other.
  • the paired surfaces may be a convex cone and a concave cone opposed to each other, or may be a convex curved surface and a concave curved surface opposed to each other.
  • connection between the shaft 713 of the motor 71 and the rotation plate 77 is not limited to the indirect connection by the magnetic attraction to rotate synchronously as described above, and may be a direct or mechanical connection so as to rotate synchronously.
  • the controller 17 and the integrated controller 17S are each a multi-purpose microcomputer, for example.
  • a computer program may be installed on each of the controller 17 and the integrated controller 17S.
  • the controller 17 and the integrated controller 17S can exert the functions described above when the computer program is executed.
  • a processing circuit implementing the functions of each of the controller 17 and the integrated controller 17S may include a device such as a programmed processor, an electrical circuit, and an application-specific integrated circuit (ASIC), or further include circuit constituent elements arranged to execute the described functions.
  • the display 12 and the integrated display 121 may be a liquid crystal display (LCD), an organic electro-luminescence (EL) display, or an inorganic EL display.

Landscapes

  • General Physics & Mathematics (AREA)
  • Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
  • Investigating Strength Of Materials By Application Of Mechanical Stress (AREA)
  • Force Measurement Appropriate To Specific Purposes (AREA)
  • A Measuring Device Byusing Mechanical Method (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
EP19834300.6A 2018-07-11 2019-07-11 Viscometer Active EP3822614B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2018131568A JP7162330B2 (ja) 2018-07-11 2018-07-11 粘度計
PCT/JP2019/027486 WO2020013273A1 (ja) 2018-07-11 2019-07-11 粘度測定ユニット及び粘度計

Publications (3)

Publication Number Publication Date
EP3822614A1 EP3822614A1 (en) 2021-05-19
EP3822614A4 EP3822614A4 (en) 2022-03-23
EP3822614B1 true EP3822614B1 (en) 2024-01-03

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EP19834300.6A Active EP3822614B1 (en) 2018-07-11 2019-07-11 Viscometer

Country Status (8)

Country Link
US (1) US11474015B2 (ko)
EP (1) EP3822614B1 (ko)
JP (1) JP7162330B2 (ko)
KR (1) KR20210029211A (ko)
CN (1) CN215115732U (ko)
PH (1) PH12021550002A1 (ko)
TW (1) TWI819025B (ko)
WO (1) WO2020013273A1 (ko)

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JPS5899650U (ja) * 1981-12-26 1983-07-06 株式会社東洋精機製作所 ゴム等の粘度測定装置
JPH0610650B2 (ja) * 1984-11-30 1994-02-09 株式会社島津製作所 粘度測定装置
US4622846A (en) * 1985-11-05 1986-11-18 Halliburton Company Consistency and static gel strength measuring device and method
JPH0772710B2 (ja) * 1987-04-25 1995-08-02 日本合成ゴム株式会社 粘弾性測定装置
JPH0740202Y2 (ja) * 1990-01-29 1995-09-13 株式会社トキメック 回転式粘度計
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JPH0735671A (ja) * 1993-07-21 1995-02-07 Enplas Corp 粘性測定装置
JP3475019B2 (ja) 1995-08-25 2003-12-08 東機産業株式会社 回転粘度計
JP3503341B2 (ja) 1996-05-31 2004-03-02 株式会社島津製作所 粘度測定装置
JPH10206252A (ja) * 1997-01-20 1998-08-07 Sony Corp 歪ゲージを用いたトルクセンサーのリニアリティ補正方法及び装置
EP1064938A1 (en) * 1999-06-28 2001-01-03 Sanofi-Synthelabo Pharmaceutical dosage forms for controlled release producing at least a timed pulse
JP3494112B2 (ja) 2000-03-27 2004-02-03 株式会社島津製作所 粘度測定装置
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CN101936868B (zh) 2010-08-03 2012-09-26 中海油田服务股份有限公司 一种便携式稠化仪
ES2388846B2 (es) * 2011-03-21 2013-06-04 Universidad De Huelva Dispositivo para la medida de propiedades reológicas y seguimiento de procesos a presión.
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JP2018131568A (ja) 2017-02-16 2018-08-23 旭化成株式会社 ポリオキシメチレン樹脂組成物及び成形体

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Publication number Publication date
JP2020008491A (ja) 2020-01-16
WO2020013273A1 (ja) 2020-01-16
US20210293684A1 (en) 2021-09-23
TW202012906A (zh) 2020-04-01
KR20210029211A (ko) 2021-03-15
CN215115732U (zh) 2021-12-10
EP3822614A1 (en) 2021-05-19
EP3822614A4 (en) 2022-03-23
TWI819025B (zh) 2023-10-21
JP7162330B2 (ja) 2022-10-28
PH12021550002A1 (en) 2021-09-20
US11474015B2 (en) 2022-10-18

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